CN105420511B - A kind of method for reducing osmium absorbing liquid - Google Patents
A kind of method for reducing osmium absorbing liquid Download PDFInfo
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- CN105420511B CN105420511B CN201510797548.8A CN201510797548A CN105420511B CN 105420511 B CN105420511 B CN 105420511B CN 201510797548 A CN201510797548 A CN 201510797548A CN 105420511 B CN105420511 B CN 105420511B
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- osmium
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- absorption liquid
- oxidant
- absorbing liquid
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- 239000007788 liquid Substances 0.000 title claims abstract description 131
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910052762 osmium Inorganic materials 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000010521 absorption reaction Methods 0.000 claims abstract description 59
- 239000007800 oxidant agent Substances 0.000 claims abstract description 25
- 230000009467 reduction Effects 0.000 claims abstract description 24
- KXTKFKPHDLXHPU-UHFFFAOYSA-N [Os].[Na] Chemical compound [Os].[Na] KXTKFKPHDLXHPU-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004821 distillation Methods 0.000 claims abstract description 19
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 230000001590 oxidative effect Effects 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000007792 addition Methods 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 9
- 239000011707 mineral Substances 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 9
- 230000009471 action Effects 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 229910000820 Os alloy Inorganic materials 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 3
- XUXNAKZDHHEHPC-UHFFFAOYSA-M sodium bromate Chemical compound [Na+].[O-]Br(=O)=O XUXNAKZDHHEHPC-UHFFFAOYSA-M 0.000 claims description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 229940079827 sodium hydrogen sulfite Drugs 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 238000005352 clarification Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 7
- 239000002244 precipitate Substances 0.000 abstract description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 abstract description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000510 noble metal Inorganic materials 0.000 abstract description 3
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 abstract description 2
- 229930003268 Vitamin C Natural products 0.000 abstract description 2
- 230000036571 hydration Effects 0.000 abstract description 2
- 238000006703 hydration reaction Methods 0.000 abstract description 2
- 238000011946 reduction process Methods 0.000 abstract description 2
- 238000004062 sedimentation Methods 0.000 abstract description 2
- 235000019154 vitamin C Nutrition 0.000 abstract description 2
- 239000011718 vitamin C Substances 0.000 abstract description 2
- GIDFDWJDIHKDMB-UHFFFAOYSA-N osmium ruthenium Chemical compound [Ru].[Os] GIDFDWJDIHKDMB-UHFFFAOYSA-N 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000005406 washing Methods 0.000 description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 3
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 238000006356 dehydrogenation reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- FIKZVFDEWIQMMQ-UHFFFAOYSA-N [Ir].[Os].[Rh] Chemical compound [Ir].[Os].[Rh] FIKZVFDEWIQMMQ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910001927 ruthenium tetroxide Inorganic materials 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
A kind of method for reducing osmium absorbing liquid, it is that the mineral obtained after enrichment containing osmium alloy or containing osmium are formed into feed liquid by pulp, under the action of oxidant, absorb by Alkali absorption liquid to obtain an osmium absorbing liquid after distillation, the osmium sodium salt that osmium absorbing liquid is obtained after reduction, the addition oxidant heating of osmium sodium salt carries out the double absorption liquid that second distillation is absorbed by Alkali absorption liquid, obtained double absorption liquid adds VC precipitation metal osmiums after adjusting material liquid pH, cooling and standings, treat that top is clarified, separation of solid and liquid substantially without suspension black particle when, draw up clear liquid, pure water is repeatedly added to neutrality, filtering, drying, calcined, hydrogen reduction is up to product osmium powder.The present invention has the following advantages：The sedimentation time greatly shortens after can making reduction by adding vitamin C, and the hydration hydrazine reaction that compares with the VC that the yield of noble metal 2. this method uses in reduction process of improving labor efficiency is slow, is easy to control；3. precipitate reduction osmium is thorough, obtained osmium powder purity is more than 99.9%.
Description
Technical field
The invention belongs to wet-treating to contain the rich osmium material work of the alloy of osmium or the mineral containing osmium after enrichment is extracted
Skill technical field, and in particular to a kind of method of the black reduction osmium absorbing liquid of reduction purification osmium in absorbing liquid from osmium.
Background technology
At present, the domestic rich platinum group metal material recycle osmium ruthenium for mainly containing osmium ruthenium using wet-treating, main process are
The OsO that the osmium ruthenium in feed liquid is oxidized to high-valence state by strong oxidizer is added first into the material containing osmium after pulp4、RuO4, and
Evaporate from feed liquid under high temperature, by accessing absorption plant, be absorbed into respectively in soda acid absorbing liquid, absorption obtains once
Osmium absorbing liquid.Osmium absorbing liquid is distilled by precipitate reduction, secondary oxidation, the double absorption liquid obtained after absorbing again, will
It is black that it with hydrazine hydrate reduction obtains osmium.This process is after using hydrazine hydrate reduction double absorption liquid, and solution is clarified by precipitation, so
And this process is difficult that osmium ruthenium precipitates completely using the method that hydrazine hydrate reduction precipitates, above left floating for a long time in liquid
The osmium of a large amount of fine particles is black, influences the progress of production efficiency and manufacturing schedule；The little particle osmium shadow of suspension in liquid at the same time
Yield index has been rung, and has not had suitable process suspension in the later stage, in order to solve the problems, such as this, has been developed a kind of efficient
Osmium absorbing liquid restoring method, it appears critically important.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of efficient reduction osmium the shortcomings that being directed in the prior art
The method of absorbing liquid.
Adopted the following technical scheme that to solve the technical problem of the present invention：
A kind of method for reducing osmium absorbing liquid, its technique are that the mineral obtained after enrichment containing osmium alloy or containing osmium are passed through slurry
Change forms feed liquid, absorbs by Alkali absorption liquid to obtain an osmium absorbing liquid under the action of oxidant, after distillation, and an osmium is inhaled
The osmium sodium salt that liquid obtains after reduction is received, the addition oxidant heating of osmium sodium salt carries out second distillation and absorbed by Alkali absorption liquid
The double absorption liquid arrived, obtained double absorption liquid add VC precipitation metal osmiums after adjusting material liquid pH, and cooling and standings, treat that top is clear
Clearly, separation of solid and liquid substantially without suspension black particle when, draw up clear liquid, repeatedly add pure water to neutrality, filter, drying, into
Row calcining, hydrogen reduction are up to product osmium powder.
A kind of method for reducing osmium absorbing liquid, its step are：
Step a, the rich osmium material of the alloy containing osmium or the mineral containing osmium after enrichment is extracted is formed into osmium absorbing liquid,
Under the action of sodium chlorate or sodium bromate oxidant, after 80-85 DEG C of distillation of high temperature, absorb to obtain an osmium suction by Alkali absorption liquid
Receive liquid；
Step b, sulfur dioxide is passed through in an osmium absorbing liquid at room temperature or adds sodium hydrogensulfite solid or saturation Asia
Sodium bisulfate, reaches 6-7 reactions in pH value and terminates, obtain osmium sodium salt；
Step c, it is 5mol/L that osmium sodium salt enriching sulfuric acid after water slurry, which controls pulp liquid acidity, is slowly added mass fraction
H2O2 oxidants or mass fraction for 30% are 30% sodium chlorate solution's oxidant, are warming up to 80-85 DEG C of progress second distillation, lead to
Cross lye to absorb to obtain double absorption liquid, the pH value with hydrochloric acid tune double absorption liquid is 1-1.5, and double absorption liquid is using VC come also
Original, VC additions are subject between deoxidization terminal to pH value reaches 6-7, and cooling, treats that top is clarified, draw up clear liquid, repeatedly add
Pure water stands filtering to neutrality, drying, is calcined, hydrogen reduction is up to product osmium powder.
Alkali absorption liquid is the KOH solution or mass fraction 10%- of mass fraction 10%-30% in the step a and step c
Add absolute ethyl alcohol in 30% NaOH solution, the mass fraction of absolute ethyl alcohol is 2%.
The adding rate of oxidant is 2L/h in the step c.
The step c is that to control pulp liquid acidity be 5mol/L to osmium sodium salt enriching sulfuric acid after water slurry, is slowly added matter
The H2O2 oxidants or mass fraction that amount fraction is 30% are 30% sodium chlorate solution's oxidant, colourless for eventually with thiocarbamide testing result
Point, the adding rate of oxidant is 2L/h, is warming up to 80-85 DEG C of progress second distillation, the secondary suction obtained by Alkali absorption liquid
Receive liquid, when double absorption liquid concentration buildup to when having a small amount of crystallization precipitation, swapped out, then by subsequent absorption device successively before
Moving, be 1-1.5 with hydrochloric acid tune pH value when the amount of double absorption liquid reaches more than 10L, double absorption liquid is reduced using VC,
VC additions are subject between deoxidization terminal to pH value reaches 6-7, and cooling, treats that top is clarified, draw up clear liquid, repeatedly add pure water
Washing stands filtering to neutrality, drying, is calcined, hydrogen reduction is up to product osmium powder.
A kind of method for reducing osmium absorbing liquid provided by the invention, has the following advantages：1. it can be made by adding vitamin C
The sedimentation time greatly shortens after reduction, the yield improved labor efficiency with noble metal；2. the VC that this method uses in reduction process
The hydration hydrazine reaction that compares is slow, is easy to control；3. precipitate reduction osmium is thorough, the standard of efflux wastewater can be reached, obtained
Osmium powder purity is more than 99.9%.
Brief description of the drawings
Fig. 1 is present invention process flow chart.
Embodiment
Embodiment 1
A kind of method for reducing osmium absorbing liquid, by the rich osmium of the alloy containing osmium or the mineral containing osmium after enrichment is extracted
Material forms osmium absorbing liquid, under the action of sodium chlorate oxidant, after 85 DEG C of distillations of high temperature, absorbs to obtain one by Alkali absorption liquid
Secondary osmium absorbing liquid；One time osmium absorbing liquid is beaten to 500L kettles, and an osmium absorbing liquid pH value is 13, leads to SO at room temperature2To pH value
Terminate in 6 reactions, be warming up to 75 DEG C, cold filtration, obtains osmium sodium salt, and the washing of osmium sodium salt is removed sodium ion therein.Osmium sodium
It is 5mol/L that salt enriching sulfuric acid after water slurry, which controls pulp liquid acidity, and mass fraction is slowly added as 30% using the speed of 2L/h
H2O2Oxidant, heat up 80 DEG C of progress second distillations, absorbs to obtain double absorption liquid, the secondary suction of follow-up level-one by lye
Liquid concentration buildup is received to when having a small amount of crystallization precipitation, is swapped out, then subsequent absorption device is moved forward successively, treats double absorption liquid
Amount when reaching 15L, be 1 with hydrochloric acid double absorption liquid pH value, double absorption liquid is reduced using VC, is reduced with the addition of VC
Terminal pH=6, stop add, cooling and standings, treat top clarify, separation of solid and liquid substantially without suspension black particle when, the time is about
61min, draws up clear liquid, and it is 6 repeatedly to add pure water to pH, is filtered, drying, is calcined, hydrogen reduction goes out by setup program
Dehydrogenation is more than 99.9% up to product osmium powder, its purity.
The Alkali absorption liquid wherein used twice is to add anhydrous C in 10% KOH solution of mass fraction2H5OH solution, anhydrous second
The mass fraction of alcohol is 2%.
Embodiment 2
A kind of method for reducing osmium absorbing liquid, by the rich osmium of the alloy containing osmium or the mineral containing osmium after enrichment is extracted
Material forms osmium absorbing liquid, under the action of sodium bromate oxidant, after 80 DEG C of distillations of high temperature, absorbs to obtain one by Alkali absorption liquid
Secondary osmium absorbing liquid；One time osmium absorbing liquid is beaten to 500L kettles, and one time osmium absorbing liquid pH value is 14, adds bisulfite at room temperature
Sodium solid terminates to pH value for 6.5 reactions, is warming up to 85 DEG C, and cold filtration, obtains osmium sodium salt, and the washing of osmium sodium salt is removed wherein
Sodium ion.It is 5mol/L that osmium sodium salt enriching sulfuric acid after water slurry, which controls pulp liquid acidity, is slowly added with the speed of 2L/h
Mass fraction is 30% sodium chlorate solution, and heat up 85 DEG C of progress second distillations, absorbs to obtain double absorption liquid by lye.Use salt
Sour double absorption liquid pH value is 1.5, and double absorption liquid is reduced using VC, with addition deoxidization terminal pH=7 of VC, stops adding
Enter, cooling and standings, treat top clarify, separation of solid and liquid substantially without suspension black particle when, time about 55min, draws up clear liquid, more
Secondary addition pure water is filtered, drying to neutrality, is calcined by setup program, hydrogen reduction goes out dehydrogenation up to product osmium powder, its
Purity is more than 99.95%.
The Alkali absorption liquid wherein used twice is to add anhydrous C in 30% NaOH solution of mass fraction2H5OH solution, it is anhydrous
The mass fraction of ethanol is 2%.
Embodiment 3
A kind of method for reducing osmium absorbing liquid, by the rich osmium of the alloy containing osmium or the mineral containing osmium after enrichment is extracted
Material forms osmium absorbing liquid, under the action of sodium chlorate oxidant, after 80 DEG C of distillations of high temperature, absorbs to obtain one by Alkali absorption liquid
Secondary osmium absorbing liquid；One time osmium absorbing liquid is beaten to 500L kettles, and an osmium absorbing liquid pH value is 14, adds saturation sulfurous at room temperature
Sour hydrogen sodium solution terminates to pH value for 7 reactions, is warming up to 85 DEG C, and cold filtration, obtains osmium sodium salt, and the washing of osmium sodium salt is removed it
In sodium ion.It is 5mol/L that osmium sodium salt enriching sulfuric acid after water slurry, which controls pulp liquid acidity, is slowly added with the speed of 2L/h
Add the H that mass fraction is 30%2O2Oxidant, heat up 85 DEG C of progress second distillations, absorbs to obtain double absorption liquid by lye, after
Continuous level-one double absorption liquid concentration buildup is swapped out to when having a small amount of crystallization to separate out, then by subsequent absorption device successively before
Move, be 1.5 with hydrochloric acid double absorption liquid pH value, double absorption liquid is using VC come also when the amount of double absorption liquid reaches 11L
Original, with addition deoxidization terminal pH=6 of VC, stops adding, cooling and standings, treats that top is clarified, separation of solid and liquid is substantially black without suspending
During coloured particles, time about 60min, draws up clear liquid, and it is 6 repeatedly to add pure water to pH, is filtered, drying, by setup program
Calcined, hydrogen reduction goes out dehydrogenation and is more than 99.93% up to product osmium powder, its purity.
The Alkali absorption liquid wherein used twice is to add anhydrous C in 30% KOH solution of mass fraction2H5OH solution, anhydrous second
The mass fraction of alcohol is 2%.
The application example of this patent：After this technology has been successfully applied to the noble metal concentrate distillation absorption osmium ruthenium containing rhodium iridium
Osmium absorbing liquid, output purity is more than 99.9% osmium powder, meets osmium powder industry quality standard（YS/T681-2008）, even
Reach 99.95% standard（SM-Os99.95）.
Claims (4)
- A kind of 1. method for reducing osmium absorbing liquid, it is characterised in that：The mineral obtained after enrichment containing osmium alloy or containing osmium are passed through Pulp forms feed liquid, absorbs by Alkali absorption liquid to obtain an osmium absorbing liquid under the action of oxidant, after distillation, by an osmium The osmium sodium salt that absorbing liquid obtains after reduction, the addition oxidant heating of osmium sodium salt carry out second distillation and are absorbed by Alkali absorption liquid Obtained double absorption liquid, obtained double absorption liquid add VC precipitation metal osmiums after adjusting material liquid pH, and cooling and standings, treat top Clarification, separation of solid and liquid substantially without suspension black particle when, draw up clear liquid, repeatedly add pure water to neutrality, filter, drying, Calcined, hydrogen reduction up to product osmium powder, concretely comprise the following steps：Step a, the rich osmium material of the alloy containing osmium or the mineral containing osmium after enrichment is extracted is formed into osmium absorbing liquid, in chlorine Under the action of sour sodium or sodium bromate oxidant, after 80-85 DEG C of distillation of high temperature, absorb to obtain an osmium absorption by Alkali absorption liquid Liquid；Step b, sulfur dioxide is passed through in an osmium absorbing liquid at room temperature or adds sodium hydrogensulfite solid or saturation sulfurous acid Hydrogen sodium solution, reaches 6-7 reactions in pH value and terminates, obtain osmium sodium salt；Step c, it is 5mol/L that osmium sodium salt enriching sulfuric acid after water slurry, which controls pulp liquid acidity, and being slowly added mass fraction is 30% H2O2Oxidant or mass fraction are 30% sodium chlorate solution's oxidant, are warming up to 80-85 DEG C of progress second distillation, pass through Lye absorbs to obtain double absorption liquid, and the pH value with hydrochloric acid tune double absorption liquid is 1-1.5, and double absorption liquid is using VC come also Original, VC additions are subject between deoxidization terminal to pH value reaches 6-7, and cooling, treats that top is clarified, draw up clear liquid, repeatedly add Pure water stands filtering to neutrality, drying, is calcined, hydrogen reduction is up to product osmium powder.
- A kind of 2. method for reducing osmium absorbing liquid according to claim 1, it is characterised in that：In the step a and step c Alkali absorption liquid is in the KOH solution of mass fraction 10%-30% or the NaOH solution of mass fraction 10%-30% plus absolute ethyl alcohol, The mass fraction of absolute ethyl alcohol is 2%.
- A kind of 3. method for reducing osmium absorbing liquid according to claim 1 or 2, it is characterised in that：Aoxidized in the step c The adding rate of agent is 2L/h.
- A kind of 4. method for reducing osmium absorbing liquid according to claim 1 or 2, it is characterised in that：The step c is osmium sodium It is 5mol/L that salt enriching sulfuric acid after water slurry, which controls pulp liquid acidity, is slowly added the H that mass fraction is 30%2O2Oxidant or Mass fraction is 30% sodium chlorate solution's oxidant, colourless for terminal with thiocarbamide testing result, and the adding rate of oxidant is 2L/ H, is warming up to 80-85 DEG C of progress second distillation, the double absorption liquid obtained by Alkali absorption liquid, treats double absorption liquid concentration buildup To when thering is a small amount of crystallization to separate out, swapped out, then subsequent absorption device is moved forward successively, treat that the amount of double absorption liquid reaches 10L It is 1-1.5 with hydrochloric acid tune pH value during the above, double absorption liquid is reduced using VC, and VC additions are reached with deoxidization terminal to pH value To subject between 6-7, cooling, treats that top is clarified, draws up clear liquid, repeatedly addition pure water to neutrality, standing filtering, drying, Calcined, hydrogen reduction is up to product osmium powder.
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